The focused output of a pulsed ruby laser is used for the in-situ pyrolysis of individual coal macerals. This study couples laser pyrolysis with gas chromatography/mass spectrometric analysis allowing for the detection of neutral, volatile organic compounds formed in coal pyrolysis. Typically, released pyrolyzates from the vitrinite of a subbituminous coal and a coalified log of lignite rank include a wide distribution of aliphatic compounds (predominantly alkanes) in addition to aromatic compounds such as alkylbenzenes, phenols, and naphthalenes. The production of such compounds highlights the efficiency of laser radiation as a source for coal pyrolysis. The distribution of the detected components in the pyrograms is typical of compounds produced from vitrinite-rich coals by other pyrolysis methods. Differing pyrolyzates populations, including subtle intensity fluctuations for common product classes, allows for chemical distinction between the two samples examined. The potential of this technique for the in-situ chemical investigation of individual coal macerals which may be present in very small amounts within the parent coal is established.